High-performance Liquid Chromatography-diode Array Research Articles

Comparative Pharmacokinetic Study of Standard Astaxanthin and its Micellar Formulation in HealthyMale Volunteers.

Astaxanthin is a naturally occurring carotenoid with high anti-oxidant properties, but it is a very lipophilic compound with low oral bioavailability. This study was conducted to compare the pharmacokinetic parameters of a novel astaxanthin preparation based on micellar solubilization technology, NovaSOL® 400-mg capsules (Test product), and those of astaxanthin 400-mg capsules (reference product), after single oral dose administration to healthy male adults. A single oral dose (400 mg equivalent to 8 mg astaxanthin) of test and reference astaxanthin were administered with 240 mL of water to 12 volunteers according to crossover design, in two phases, with a washout period of 1week in between. Blood samples were collected at hourly intervals for the first 12 h, then at 24.0, 48.0, and 72.0 h after administration. Aliquots of plasma were centrifuged and the clear supernatant was injected into the high performance liquid chromatography-diode array detection (HPLC-DAD) system. Plasma concentration of astaxanthin versus time profiles were constructed, and the primary pharmacokinetic parameters, maximum concentration (Cmax), area under concentration time curve from time of administration (0) to time (t) [AUC0-t] or to infinity ∞, [AUC0-∞], half-life (T½) and time to reach Cmax (Tmax)were calculated. The test micellar astaxanthin reached a Cmax of 7.21 µg/ml after 3.67 h compared to only 3.86 µg/ml after 8.5 h for the reference native astaxanthin. Micellar formulation of astaxanthin is capable of producing a high concentration of astaxanthin in plasma in a shorter time, thereby expected to provide faster potential therapeutic efficacy.

Gastrointestinal digestion of olive leaf waste from olive mill production chain in a simulator of the gastrointestinal tract.

Currently, olive leaves are considered waste, although their high phenolic content makes them a source of antioxidants that could be used directly. The aim of this work was to study the behavior of phenolic compounds contained in olive leaf from the olive mill production chain during their gastrointestinal digestion. Phenolic compounds in the gastric digestion analyzed by high-performance liquid chromatography-diode array detection-mass spectrometry increased by 58% to 314.5% compared to the meal, while in the intestinal stage they ranged from 1.87 to 9.04 times higher. An increase of between 187% and 903% in bioaccessibility of phenolic compounds in the intestinal phase was observed, except for verbascoside. Furthermore, such compounds were fully bioavailable, except for apigenin-7-O-glucoside, which showed a bioavailability of 56%. The current study showed that the concentration of oleuropein, apigegin-7-O-glucoside, hydroxytyrosol hexoside and hydroxytyrosol contained in olive leaf continued to be extracted during the gastrointestinal digestion process. Furthermore, the results obtained with respect to their bioaccessibility and bioavailability suggest a good disposition to pass into the bloodstream where they could exert beneficial effects. Therefore, these results are promising for olive leaf becoming a consumable by-product that could be directly ingested through a simple infusion. © 2024 The Authors. Journal of The Science of Food and Agriculture published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry.

Phenolic and Antioxidant Characterization of Fruit By-Products for Their Nutraceuticals and Dietary Supplements Valorization under a Circular Bio-Economy Approach.

Agri-food by-products, obtained as waste from the food industry, negatively impact the global economy and the environment. In order to valorize waste materials from fruit juices and tomato sauces as upcycled materials rich in health-promoting compounds, they were characterized in terms of polyphenolic and protein content. The results obtained were compared with those collected for their final products. The recovery of polyphenols was performed via ultrasound-assisted extraction (UAE). A high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed and validated to depict the quali-quantitative polyphenolic profile of both the by-products and the final products. The antioxidant capacity of the resulting extracts was characterized by UV-Vis spectrophotometric assays in terms of total phenolic content (TPC) and total antioxidant status (TAS). Moreover, the protein content was assessed with the Kjeldahl method too. The results highlighted a significant quantity of polyphenols remaining in peach, apricot, and apple by-products, which were able to exert an antioxidant activity (in the range of 4.95 ± 5.69 × 10-1 to 7.06 ± 7.96 × 10-1 mmol Trolox 100 g-1 of dry weight (DW) sample). Conversely, the tomato by-products were highly rich in proteins (11.0 ± 2.00 to 14.4 ± 2.60 g of proteins 100 g-1 DW). The results proved that all by-products may potentially be sustainable ingredients with nutritional and functional value in a circular bio-economy prospect.

Qualitative and Quantitative Analysis of Chemical Components in Yinhua Pinggan Granule with High-Performance Liquid Chromatography Coupled with Q-Exactive Mass Spectrometry.

Yinhua Pinggan Granule (YPG) is an approved compounded traditional Chinese medicine (TCM) prescription for the treatment of cold, cough, viral pneumonia, and related diseases. Due to its complicated chemical composition, the material basis of YPG has not been systematically investigated. In this study, an analytical method based on high-performance liquid chromatography (HPLC) coupled with Q-Exactive mass spectrometry was established. Together with the help of a self-built compound database and Compound Discoverer software 3.1, the chemical components in YPG were tentatively identified. Subsequently, six main components in YPG were quantitatively characterized with a high-performance liquid chromatography-diode array detector (HPLC-DAD) method. As a result, 380 components were annotated, including 19 alkaloids, 8 organic acids, 36 phenolic acids, 27 other phenols, 114 flavonoids, 75 flavonoid glycoside, 72 terpenes, 11 anthraquinones, and 18 other compounds. Six main components, namely, chlorogenic acid, puerarin, 3'-methoxypuerarin, polydatin, glycyrrhizic acid, and emodin, were quantified simultaneously. The calibration curves of all six analytes showed good linearity (R2 > 0.9990) within the test ranges. The precision, repeatability, stability, and recovery values were all in acceptable ranges. In addition, the total phenol content and DPPH scavenging activity of YPG were also determined. The systematic elucidation of the chemical components in YPG in this study may provide clear chemical information for the quality control and pharmacological research of YPG and related TCM compounded prescriptions.

UiO-66@Fe3O4 nanocomposite as an adsorbent in dispersive solid phase extraction of metformin in surface water and wastewater

Metformin, an anti-hypoglycemic medication, has been used for decades due to its efficiency and is the most consumed pharmaceutical drug worldwide. Consequently, monitoring its concentration in environmental water is important due to its suspected effect on human health and aquatic life. This study reported the extraction, preconcentration, separation and determination of metformin (MET) in waters. Dispersive solid phase extraction (dSPE) using UiO-66@Fe3O4 nanocomposite as a sorbent was used to extract and preconcentrate MET. The high-performance liquid chromatography-diode array detector (HPLC-DAD) achieved the separation and quantification of MET in the samples. Experiemental design was used to optimise influential variables in the extraction and preconcentration of MET. The linearity, limit of detection (LOD) and limit of quantification (LOQ) for MET were 0.5–100 μg L−1 (R2 = 0.9987), 0.16 μg L−1 and 0.53 μg L−1, respectively. The intraday (n = 10 same-day replicates) and interday (n = 5 consecutive days) precisions reported as relative standard deviations (RSD %) were less than 5%. The accuracy of the method expressed as percentage recovery (%R) ranged from 84 to 112%. The method was applied to extract and preconcentrate MET in wastewater and river water samples. The MET was detected in greater concentrations in wastewater than in river water samples. The validation based on specificity, trueness, linearity, precision, and application to the analysis of MET in real samples showed that the combination of dSPE and HPLC-DAD methods is applicable for MET monitoring in surface water and wastewater. Furthermore, the dSPE/HPLC-DAD method was rapid, simple and suitable for estimating the concentrations of MET in South African surface water and wastewater for the first time. Lastly, the environmental risk caused by the occurrence of MET in surface water was investigated in terms of hazard quotient (HQ). The HQ values were less than unity, suggesting a low possibility risk for the aquatic organisms.

Development of Magnetic Solid Phase Micro-Extraction (MSPE) Method for the Extraction and Preconcentration of the Selected β-Blockers in the Environmental Wastewaters

AbstractEmerging organic pollutants s have always been the greatest environmental concern due to their ubiquity and distinguished adverse effects. These are mostly water-bone pollutants flagged as endocrine disruptors and can greatly inconvenience the ecosystem. Among others, β-blockers have also been detected in the environment at various concentrations that threaten the well-being of humans and animals. In this work, NH2-MIL-101(Cr) doped magnetic nanoparticles nanocomposite was successfully synthesised and characterised using analytical techniques such as X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET) and transmission electron microscopy (TEM). The Fe3O4@NH2-MIL-101(Cr) was then used as an adsorbent to extract the selected β-blockers in the environmental wastewater. The selected β-blockers were quantified using a high-performance liquid chromatography-diode array detector (HPLC-DAD). Parameters affecting the extraction were screened and optimised using fractional factorial design (FFD) and central composite design (CCD), respectively. Under optimum conditions, the LODs were 0.057 and 0.065 µg L− 1, and LOQs were 0.19 and 0.22 µg L− 1 for acebutolol (ACE) and metoprolol (MET), respectively. The calibration curve exhibited the linearity range of 0.2–1200 µg L− 1 with correlation coefficients of 0.9987 and 0.9968 for ACE and MET, respectively. Repeatability studies demonstrated the %RSD of 0.63 and 0.74% for MET and ACE. At the same time, reproducibility studies displayed the %RSD of 1.057 and 1.178% for MET and ACE, respectively. Spike recovery experiments were carried out to assess the performance of MSPE in real samples, and over 88% of both analytes were recovered. This indicated that the MSPE method could enrich various organic pollutants from different environmental matrices.

Melamine sponges incorporated azo-linked porous organic polymer as adsorbent for extraction and determination of six B vitamins using pipette tip micro solid-phase extraction

A novel azo-linked porous organic polymer (AL-POP) was synthesized from caffeic acid and benzidine via an azo-coupling reaction and characterized by FTIR, SEM-EDS, BET, TGA, XRD and zeta potential analysis. AL-POPs were incorporated into melamine sponges and used for pipette tip micro solid-phase extraction (PT-MSPE) of six types of B vitamins (including thiamine, riboflavin, nicotinamide, pyridoxine, folic acid, and cyanocobalamin). After extraction, the samples were analyzed using high performance liquid chromatography-diode array detection (HPLC-DAD) system. The effect of AL-POP composition on the extraction efficiency (EE) of vitamins was investigated and benzidine to caffeic acid mol ratio of 1.5, 3.35 mmol of NaNO2, and reaction time of 8 h were selected as optimum conditions. The efficiency of the extraction process was improved by optimizing various parameters such as the amount of sorbent, pH and ionic strength of the sample, sample volume, number of adsorption and desorption cycles, type of wash solvent, and type and volume of eluent solvent. Linearity (R2≥0.9987), Limit of detection (LOD) (11.88-18.97 ng/mL), limit of quantification (LOQ) (39.62-63.23 ng/mL), and enrichment factor (EF) (1.27-4.31)) were obtained using calibration curves plotted under optimum conditions. Recovery values of these six B vitamins in the spiked multivitamin syrup samples varied from 80.01% to 108.35%, with a relative standard deviation (RSD) below 5.44%. Eventually, the optimized method was successfully used to extract and quantify the B vitamins in multivitamin syrup and non-alcoholic beer.

Quantification of phenolic compounds in dietary supplements and antioxidant activities

Dietary supplements (DS) are products that are recommended for the treatment of various health issues, especially during the global pandemic, and the accuracy of the labeling information of these supplements plays a significant role in human health. In this study, a novel high performance liquid chromatography-diode array detector (HPLC-DAD) method was developed and validated to determine the accuracy of the labeling information of commercial dietary supplements containing phenolic compounds (rutin, quercetin, and resveratrol). The mobile phase, flow rate, and column temperature were optimized. Validation studies were carried out to prove the validity of the developed method. The limit of detection (LOD) and limit of quantification (LOQ) values ​​of rutin, quercetin, and resveratrol were found in the range of 4.83-6.62 ng/mL and 16.09-22.07 ng/mL, respectively. Recoveries% were calculated in the range of 99.52-100.19% and 99.78-100.34% in the intra-day and inter-day analysis, respectively. The IC50 values of the dietary supplement extracts obtained by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) method ranged from 0.08 to 0.76 mg/mL. Total Antioxidant Capacity (TAC) values of DS1, DS2, DS3, DS4, DS5, measured employing the Cupric Reducing Antioxidant Capacity (CUPRAC) method, were found to be 0.09, 0.03, 0.10, 0.10 and 0.40 mmol trolox per gram of extract, respectively. KEY WORDS: Dietary supplement, HPLC-DAD, Phenolic compound, Antioxidant activity Bull. Chem. Soc. Ethiop. 2024, 38(4), 853-862. DOI: https://dx.doi.org/10.4314/bcse.v38i4.3

Antimicrobial and Antiplasmodial Activities of Endophytic Fungi Associated with Psidium guajava

Infections due to antimicrobial-resistant microorganisms have become widespread in recent years. Thus, searching for novel antimicrobial agents to combat such pathogens has become crucial. The current study aimed to evaluate the antimicrobial, antiplasmodial, and immunomodulatory activities of the extracts of endophytic fungi isolated from Psidium guajava. Isolation, identification, fermentation, and extraction of the secondary metabolites of the fungal endophytes were carried out following standard procedures. The extracts were subjected to High-Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD) analysis to detect their bioactive components. The Antimicrobial activity and Minimum Inhibitory Concentration of the fungal extracts were evaluated against pure cultures of Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa, Salmonella typhi, and Klebsiella pneumonia using Agar well diffusion and Agar dilution method respectively. The acute toxicity study (LD50) was carried out using Lorke’s method. The extracts were tested in vivo in mice for antiplasmodial activity against Plasmodium berghei and in vitro against Plasmodium falciparum using Peter and Reyley's curative test method and WHO standardized micro-test system with modification respectively. The immunomodulatory activity of the extracts was evaluated by cyclophosphamide-induced myelosuppression (hematological parameters). Active extracts were further subjected to Delayed-Type Hypersensitivity Response (DTHR) and Haemagglutination Inhibition Assay using Sheep Red Blood Cells as antigens. The result showed Alternaria sp. (PGL1, PGL2, PGL3), from P. guajava. The HPLC-DAD analysis revealed the presence of bioactive compounds previously reported to have antimicrobial, antiplasmodial, and immunomodulatory properties. The fungal extracts exhibited varying degrees of antimicrobial activity. The LD50 of the fungi extracts was>5000 mg/kg in mice. The extracts at 100 and 200 mg/kg body weight in mice showed varying degrees of antiplasmodial activity. Growth of P. berghei was significantly (p<0.001) inhibited, curative effect ranges from 59.09 – 100%. Schizont maturation of P. falciparum isolates was inhibited and the highest level of inhibition was observed at 1 mg/ml (p<0.05). The fungal extracts reversed the effect of cyclophosphamide-induced reduction in total white blood cell counts and % neutrophil. This study showed that the tested plant harbors species of endophytic fungi that contain numerous secondary metabolites. The endophytic fungi showed prophylactic, immunostimulatory, and antiplasmodial activities, which can be exploited to develop antimicrobial, antiplasmodial, and immunomodulatory agents.

Application of continuous magnetic solid phase extraction in the extraction of tetracycline antibiotics from honey samples

This study aimed to develop a continuous magnetic solid phase extraction method in a narrow bore tube for the extraction of tetracycline antibiotics from honey samples before their determination with high performance liquid chromatography–diode array detector. In this work, a magnetic covalent organic framework is used as the sorbent. The extraction method is performed in a narrow bore tube by adding 25 mg of a magnetic sorbent prepared from melamine, barbituric acid, and Fe3O4 into the diluted honey sample solution. By using a magnet, the sorbent is moved up and down through the narrow bore tube for five times to improve extraction efficiency. After adsorption the analytes, they are eluted from the sorbent surface using 2,2–dimethoxypropane under vortexing. Then, by using a magnet, the eluent containing the extracted analytes are taken and evaporated with continuous flow of nitrogen. Finally, the residue containing the enriched analytes is reconstituted in microliter–level of mobile phase and injected into chromatographic system for quantitative analysis. Based on the outcomes, the method demonstrated good linearity (0.37–1000 ng g−1), high enrichment factors (175–203), good extraction recoveries (70–81 %), low LODs (0.11–0.18 ng g−1) and LOQs (0.37–0.60 ng g−1). The proposed method is effectively applied for quantification of tetracyclines in twenty–four honey samples. Considering the results, none of the honey samples was contaminated with the studied antibiotics. Regarding to the above–mentioned analytical advantages of the proposed method, its simplicity and rapidity, and green synthesis of the magnetic sorbent particles, the suggested method can be used as a routine method for the extraction of tetracyclines from honey samples.

Evaluation of some sulfonamide antibiotics residues in chicken meat samples using in-syringe counter current homogenous liquid–liquid extraction and magnetic deep eutectic solvent-based dispersive liquid–liquid microextraction and HPLC–DAD

A sample pretreatment method based on the combination of counter current salting-out homogenous liquid–liquid extraction and magnetic deep eutectic solvent-based dispersive liquid–liquid microextraction was developed and employed for the extraction of some sulfonamide antibiotics from chicken meat samples. For this purpose, first, a homogenous solution of acetonitrile and deionized water was passed through a syringe barrel filled sodium chloride and chicken meat sample. By doing so, the fine droplets of acetonitrile were produced and collected on the surface of solution. In the following, this phase containing the extracted analytes was taken and injected into deionized water after mixing with [Choline: 4-chlorophenol]+[FeCl4]- magnetic deep eutectic solvent. Then, the magnetic deep eutectic solvent droplets were separated in the presence of an external magnetic field and injected into high performance liquid chromatography-diode array detector for quantitative analysis. Based on the validation results, low limits of detection (0.15–0.24 ng g−1) and quantification (0.51–0.80 ng g−1), high extraction recovery (67–78 %), and good precision (relative standard deviations ≤ 5.7 %) were obtainable by using the offered method. Finally, the suggested method was employed for the quantification of the studied sulfonamide antibiotics in various chicken meat samples.

Towards an index of damage of olive paste during virgin olive oil extraction: The role of β-OH-acteoside diastereomers for risk assessment of the fusty/muddy sediment sensory defect

The aim of this study was to propose an index/marker of thermal/oxidative damage of olive paste during virgin olive oil extraction to assess the risk of sensory defects in the obtained oil. Several olive oil extraction trials were carried out over two production years applying different time, temperature, and oxygen exposure conditions during malaxation. The phenolic composition of the olive pastes was analyzed by High Performance Liquid Chromatography-Diode Array Detector-Mass Spectrometry (HPLC-DAD-MS). The chemical (legal quality indexes, phenolic compounds by HPLC-DAD-MS, volatile compounds by Head Space-Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS)) and sensory characteristics of the obtained oils were analyzed. The content of the β-OH-acteoside diastereomers in olive paste increased linearly with malaxation time as a function of malaxation temperature and oxidative conditions, following a pseudo-zero order kinetic. At the same time, two volatile compounds linked to sensory defects (2- and 3-methylbutanal) increased in the obtained oils when increasing malaxation time and temperature, and a relationship between them and the fusty/muddy sediment defect in olive oil samples was observed. A further direct relationship between the β-OH-acteoside content in the olive pastes and the 2+3-methylbutanal content in the oils was observed. Therefore, the β-OH-acteoside diastereomers content in olive pastes has been suggested as an index/marker to indicate the risk of sensory defects in virgin olive oil as a function of the thermal and oxidative conditions during malaxation. A threshold value of 100 mg/kg of the content of β-OH-acteoside diastereomers was proposed, above which the fusty/muddy sediment defect is perceptible.

Simultaneous extraction of polycyclic aromatic hydrocarbons and tetracycline antibiotics from honey samples using dispersive solid phase extraction combined with dispersive liquid-liquid microextraction before their determination with HPLC-DAD

A dispersive solid-phase extraction method combined with dispersive liquid-liquid microextraction was offered for the extraction of four polycyclic aromatic hydrocarbons (anthracene, fluorene, phenanthrene, and pyrene) and tetracycline antibiotics (tetracycline, oxytetracycline, and chlortetracycline) from honey samples, simultaneously. In this work, cobalt-gallic acid bio-metal organic framework was synthesized and 20 mg of it was added into of 10 mL the diluted honey solution to efficiently adsorb the analytes. After vortexing (3 min) and centrifuging, the sorbent particles were eluted with 0.75 mL acetonitrile under vortexing for 3 min. In the following, this phase was mixed with 55 µL [Ch: 4-chlorophenol]+[FeCl4]- magnetic deep eutectic solvent and rapidly injected into deionized water. After separating the extractant phase in the presence of an external magnet and diluting it with the mobile phase, it was injected into a high-performance liquid chromatography-diode array detector. Under optimum extraction conditions, extraction recoveries were in the range of 63–84%. The limits of detection of the opted polycyclic aromatic hydrocarbons and tetracyclines were in the ranges of 0.18–0.26 and 0.25–0.29 ng g−1, respectively. Also, good repeatability (relative standard deviations ≤ 7.5 and 8.3% for intra– (n=6) and inter-day (n=4) precisions, respectively) was obtained. In summary, the validated method was successfully recommended for the determination of polycyclic aromatic hydrocarbons and tetracyclines in various honey samples and pyrene was found in two samples at 5.5 and 12.9 ng g−1. The used bio-metal organic framework has sufficient ability in extraction of different classes of compounds (polycyclic aromatic hydrocarbons and antibiotics) from honey. Performing the microextraction step has direct effect in analysis of the analytes in low concentrations and the use of magnetic solvents, eliminate the use of centrifugation in this step.

Chemical characterization, multivariate analysis and comparison of biological activities of different parts of Fraxinus mandshurica.

Fraxinus mandshurica (Oleaceae) is used as a traditional medicinal plant for the treatment of red eyes, menstrual disorders, excessive leucorrhea, chronic bronchitis and psoriasis. To perform chemical characterization of the secondary metabolites of F. mandshurica roots, bark, stems and leaves, 32 samples were collected from eight provinces in this study. A total of 64 chemical components were detected from four different parts of F. mandshurica by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry. Meanwhile, a total of nine secoiridoids were obtained by natural product chemical extraction, isolation and identification methods. Quantitative analysis by high-performance liquid chromatography-diode array detection-mass spectrometry showed the highest total content of secoiridoids in the bark, which is also consistent with the traditional medicinal parts. The results of methodological validation showed that the correlation coefficient (R2 ) values were all >0.9993, indicating a good linear range of the standard curve, while the relative standard deviations of precision, reproducibility and stability were <3%, and the spiked recoveries ranged from 98.22 to 102.27%, indicating that the experimental method was reliable and stable. In addition, fingerprinting and a heatmap were established to demonstrate the content trends of F. mandshurica more visually from different origins. Multivariate analysis, including principal component analysis and partial least squares discriminant analysis, was performed to determine the chemical characteristics of different parts of F. mandshurica, and six characteristic secoiridoids that could be used to distinguish different origins were screened. Finally, the inhibition of tyrosinase, α-glucosidase, acetylcholinesterase and pancreatic lipase activities by the nine characteristic compounds and extracts from different parts were investigated, and the results showed that they all exhibited different degrees of enzyme activity inhibition and thus have potential applications in whitening and blemish removal, hypoglycemia, anti-Alzheimer's disease and anti-obesity as a new source of natural enzyme activity inhibitors. This study establishes an identification and evaluation method applicable to phytochemistry of different origins, which is a guideline for quality control, origin evaluation and clinical application of traditional medicinal plants. This is also an unprecedented study on the identification of the chemical composition of different parts of F. mandshurica, characteristic compounds and the inhibition of enzyme activity of extracts from different parts.

Deep eutectic solvent-based pressurized liquid extraction combined with dispersive liquid-liquid microextraction of organophosphorus pesticide residues in egg powder prior to high-performance liquid chromatography analysis.

Herein, a deep eutectic solvent (DES)-based miniaturized pressurized liquid extraction in combination with DES-based dispersive liquid-liquid microextraction (DLLME) was developed for the extraction of organophosphorus pesticides (parathion-methyl, triazophos, parathion, diazinon, and phoxim) from egg powder samples prior to their analysis by a high-performance liquid chromatography-diode array detector. In this work, first, the analytes' extraction was done by a pressurized liquid phase extraction for effective extraction of the analytes from the solid matrix, and then they were concentrated on a DLLME for more concentration of the analytes to reach low limits of detections. The use of DESs was done in both steps to omit the use of toxic organic solvents. Satisfactory results including high extraction recoveries (74-90%), great repeatability (relative standard deviations equal or less than 4.3% and 5.3% for intra- and inter-day precisions), and low limits of detection (0.11-0.29ng/g) and quantification (0.38-0.98ng/g) were attained under the optimum conditions. Lastly, the suggested approach was utilized for the determination of the studied pesticides in various egg powder samples marketed in Tabriz, Iran.

Green synthesis of azo-linked porous organic polymer for enrichment of nitroimidazoles from water, shrimp and Basa fish

Reliable monitoring of nitroimidazoles (NDZs) is of great significance to public health. Herein, an azo-linked porous organic polymer (Res-POPs) was prepared by green synthesis method using natural resveratrol as monomer for the first time. Using Res-POPs as sorbent, a facile method coupling solid-phase extraction with high performance liquid chromatography-diode array detection was developed for effective detecting NDZs. The method achieved good linearities (0.06 ∼ 100 ng mL−1 for water, 1.8 ∼ 200 ng g−1 for shrimp, and 1.5 ∼ 200 ng g−1 for Basa fish) with determination coefficients above 0.995, low detection limits (0.02 ∼ 0.05 ng mL−1, 0.60 ∼ 1.00 ng g−1 and 0.50 ∼ 0.90 ng g−1 for water, shrimp and Basa fish), high method recovery (85 %∼114 %) and relative standard deviations below 8.2 %. The results demonstrated the superiority and the promising potential of the established method for detection of NDZs compared with the reported method.

Analysis of the Influence of Different Processing Methods on the Main Effective Components in Oviductus Ranae by High-Performance Liquid Chromatography with Diode Array Detector

Oviductus Ranae (OR) is one of the “treasures of Changbai Mountain” in China. It is used clinically for the treatment of infirmity after illness, fatigued spirit, cough, hemoptysis, and so forth. In this study, a simple and sensitive high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed for the simultaneous determination of five main effective components (1-methyl hydantoin, estradiol, cholesterol, 7-keto-cholesterol, and 4-cholesten-3-one) in OR and its different processed products. The results indicated that these five components showed good linear relationships within their own concentration ranges along with coefficients of determination ≥0.9996. Average recoveries ranged from 97.67% to 100.06%, with RSDs of 1.45%–1.99%. The proposed method was found to be simple, accurate, and stable, which provided an effective analytical method for quality control and evaluation of OR and its different processed products.

Reaction of cyclamate with hypochlorous acid in vitro and formation of chlorcyclohexylamine and cyclohexylamine

In this work, we investigated the reaction of cyclamate with hypochlorous acid (HOCl) in simulated gastric juice. The reaction products were detected by high-performance liquid chromatography diode array detection (HPLC-DAD) and ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS). We also explored the changes in product concentration as a function of reaction time, cyclamate and HOCl concentrations. Cyclamate reacted with hypochlorous acid instantly in the simulated gastric fluid. N, N-dichlorcyclohexylamine and cyclohexylamine were both detected when the HOCl concentration was at millimole. Cyclohexylamine can only be found when HOCl concentration was at micromole. N, N-dichlorcyclohexylamine and cyclohexylamine concentrations both increased when cyclamate concentration increased under the millimole level of HOCl. As an important reactive oxygen species, hypochlorous acid (HClO) is produced in various physiological processes. The abnormal rise of the HClO level is associated with many inflammatory diseases. Chronic gastritis associated with Helicobacter pylori is a multistep, progressive, life-long inflammation. So, chronic gastritis infected with H. pylori may cause cyclamate metabolizing into cyclohexylamine in vivo.

Profiling and evaluation of phenolic compounds in olive mill wastewater in Jordan

Abstract Phenolic compounds (PCs) are prevalent in olive mill wastewater (OMW), offering numerous health benefits but concurrently posing environmental challenges. This study aims to comprehensively characterize PCs in OMW, both qualitatively and quantitatively. An accurate, sensitive, and cost-effective method was successfully developed for extracting and quantifying seven PCs in OMW. The extraction procedure was optimized to achieve the maximum recovery using a liquid-liquid extraction method. Concentrations of the identified PCs were determined using a high-performance liquid chromatography-diode array detector (HPLC-DAD). The seven PCs peaks were successfully separated on an RP-C8 column within a 23-minute runtime using a gradient mobile phase. The method underwent thorough validation, producing satisfactory results. Subsequently, the developed method was applied to analyze OMW from four olive mills in Jordan, revealing PC concentrations ranging from 139 to 430 mg/L. Tyrosol and hydroxytyrosol were identified as the most abundant compounds. Additionally, gas chromatography-mass spectrometry (GC-MS) separated and identified forty PCs. The total phenolic content was quantified, reaching a value of 1839 mg/L. Moreover, the antioxidant activity was assessed, yielding a maximum value of 95.8%. These results underscore the substantial levels of PCs in OMW, highlighting the importance of economically utilizing this water.

Development of a dispersive liquid-liquid microextraction method for the determination of plastic additives in seawater.

A method using dispersive liquid-liquid microextraction (DLLME) prior to high performance liquid chromatography-diode array detection (HPLC-DAD) was developed to determine seven additives from the plastics industry (butylated hydroxytoluene, diisodecyl phthalate, irgafos 168, lawsone, quercetin, triclosan and vitamin E) in seawater samples. These compounds can reach seawater due to direct discharge from wastewater treatment plants and leaching from plastics and microplastics. The extraction was performed using 25 mL of seawater, 500 μL of 1-octanol (extraction solvent) and a stirring step instead of dispersive solvent. Additive concentrations were determined by LC-DAD on a C18 column with a mobile phase of acetonitrile and phosphoric acid aqueous solution (pH 3.5) by gradient elution. The analytical recoveries ranged from 82 to 93% for all compounds, except for lawsone (60%). Repeatability and intermediate precision were adequate with RSD < calculated values following the Horwitz equation at the concentration levels evaluated (0.06 and 0.24 mg L-1). All additives exhibited linear matrix calibration curves (R2 > 0.99). Detection limits ranged from 0.009 to 0.028 mg L-1 and quantification limits ranged from 0.027 to 0.084 mg L-1. Finally, the application of the method to real samples verified the method as accurate and applicable to seawater.